CN108195816A - The method that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots - Google Patents
The method that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots Download PDFInfo
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- CN108195816A CN108195816A CN201810113170.9A CN201810113170A CN108195816A CN 108195816 A CN108195816 A CN 108195816A CN 201810113170 A CN201810113170 A CN 201810113170A CN 108195816 A CN108195816 A CN 108195816A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6439—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" with indicators, stains, dyes, tags, labels, marks
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Abstract
The invention belongs to chemical application technology fields, and in particular to it is a kind of using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots solution and for pH value of solution detection.The method of present invention detection solution ph includes the following steps：Using phloroglucin as carbon source, under sulfuric acid medium, under microwave heating condition, carbon dots solution is synthesized, obtains the carbon dots solution with fluorescent characteristic；The carbon dots of synthesis have fluorescent characteristic, and maximum excitation wavelength is 365 nm, and maximum emission wavelength is 465 nm；Carbon dots solution from after the solution reaction of different pH, it is in a linear relationship between the logarithm of fluorescence intensity correlation ratio of carbon dots solution and the pH of solution (㏒（I F /I Fo ）=0.9283+0.3070 pH), the range of linearity of detection is 1.81 5.72.Based on this linear relationship, the concentration of acetic acid can be detected.
Description
Technical field
The invention belongs to chemical application technology fields, and in particular to one kind is using phloroglucin as carbon source microwave Fast back-projection algorithm carbon
The method of point detection pH value of solution.
Background technology
Fluorescent carbon point is one of most popular carbon nanomaterial after fullerene, carbon nanotube and graphene.This kind is received
Rice material overcomes certain shortcomings of traditional quantum dot, not only with excellent optical property and small size property, but also has
Good biocompatibility, it is easy to accomplish it is surface-functionalized, biochemical sensitive, imaging analysis, environment measuring, photocatalysis technology,
The fields such as metal ion detection and pharmaceutical carrier have good application potential.Synthetic method includes electrochemical process, and hydro-thermal method is micro-
Wave method, ultrasonic method etc..
Early stage people utilize electrochemical measurement pH value, but since the impedance of traditional glass electrode is high, cracky and not
The measure of fluorine-containing pH value in solution is preferably used for, and has " sodium error " in high alkalinity environment, electrochemistry is made to be met in pH value measurement
To many problems.Therefore, people continually develop new pH sensors in recent years, such as：Organic dyestuff, carbon dots, silicon nano dots, Tong Na
Rice cluster, quantum dot etc., but the problems such as some is there are still probe building-up process complexity, and detection method bothers.
Invention content
The main object of the present invention is that the synthesis of existing carbon dots and the detection technique of pH value of solution and method are shown
Some defects come provide a kind of method that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, this method
It is different from the fluorescent value of solution after the solution reaction of different pH using carbon dots solution, solution can be detected in the range of certain pH
PH, and this method have carbon dots aggregate velocity it is fast, pH measure it is easy to operate the characteristics of.
The technical solution adopted by the present invention：It is a kind of to detect pH value of solution by carbon source microwave Fast back-projection algorithm carbon dots of phloroglucin
Method, including step：(1) using phloroglucin as carbon source, the thick solution of carbon dots is synthesized under microwave heating condition, through centrifuging, filtering
Final carbon dots solution is obtained after processing；(2) system after detecting carbon dots solution and its being reacted from the BR buffer solutions of different pH value
Fluorescence intensity；(3) according to the relationship between the pH value of system and the logarithm of the fluorescence correlation ratio of carbon dots solution, Ke Yijian
Measure the pH of solution.
Preferably, step (1) is described using phloroglucin as carbon source, the process of carbon dots solution is synthesized under microwave heating condition
It is：The phloroglucin solution being configured is mixed in a certain ratio with certain density dilute sulfuric acid, then will be at mixed solution heating
Reason with water dissolution is the thick solution of carbon dots after reaction.
Preferably, a concentration of 3.0 mmol/L of phloroglucin, a concentration of 1mol/L of sulfuric acid, phloroglucin and dilute sulphur
The total volume of acid is 20 mL.
Preferably, mixed solution is placed in microwave heating treatment in micro-wave oven in step (1), firepower is middle high fire.
Preferably, the microwave heating treatment time is 10 min.
Preferably, the processing of step (1) carbon dots solution：First by the thick solution of obtained carbon dots be respectively placed in centrifuge tube into
Row is centrifuged at a high speed, then obtained supernatant carried out to be filtered under diminished pressure processing, and it is molten finally just to obtain the transparent carbon dots of brown color
Liquid.
Preferably, the centrifugal speed of the operation of the centrifugal treating of the thick solution of carbon dots of step (1) described acquisition is 10000
Rev/min, centrifugation time is 10 minutes.
Preferably, the ranging from 1.81-5.72 of pH value of solution can be detected.
Preferably, the carbon dots average grain diameter of synthesis is：2.90 nm.
Preferably, the carbon dots of synthesis have fluorescent characteristic, maximum excitation wavelength is 365 nm, and maximum emission wavelength is
465 nm。
It is fluorescence probe the present invention is based on newly synthesized carbon dots, the method for establishing detection pH value of solution.This method has carbon
Point aggregate velocity is fast, and pH measures the features such as easy to operate.
Description of the drawings
Fig. 1 is the fluorescence spectra of carbon dots solution prepared by the embodiment of the present invention.
Fig. 2 is the TEM figures of carbon dots solution prepared by the embodiment of the present invention.
Fig. 3 be the embodiment of the present invention prepare carbon dots solution TEM in grain size distribution.
Fig. 4 is the figure of fluorescence intensity changes that carbon dots solution prepared by the embodiment of the present invention detects different pH solution.
Fig. 5 be the fluorescence intensity correlation ratio of carbon dots solution prepared by the embodiment of the present invention logarithm and system pH it
Between linear relationship chart.
Specific embodiment：
Following embodiment is intended to further illustrate the present invention rather than limitation of the invention further.
(1) preparation of carbon dots
Phloroglucin solution and dilute sulfuric acid are pressed into 2.85mmol/L in conical flask:15mmol/L ratios mix, and conical flask is turned
It moves in micro-wave oven, middle high fire, 10 min of microwave heating.Conical flask is taken out after reaction, and with 15 mL water dissolutions, gained is molten
Liquid is the thick solution of carbon dots.The thick solution of carbon dots first with 10000 revs/min is centrifuged 10 minutes, takes supernatant, then with 0.2 μ of aperture
Carbon dots solution is obtained by filtration in the filter membrane vacuum decompression of m.As shown in Figure 1, maximum excitation wavelength is 365 nm, maximum emission wavelength is
465 nm.And pattern to carbon dots etc. has carried out TEM characterizations, as shown in Fig. 2, the carbon dots good dispersion of synthesis, and more uniformly.
Particle diameter distribution result (such as Fig. 3) shows carbon dots size in 2.90 nm or so.
(2) the preparation condition optimization of carbon dots
Total volume, the microwave for having inquired into the concentration of phloroglucin solution, the concentration of dilute sulfuric acid, phloroglucin solution and dilute sulfuric acid add
Influence of the firepower and the volume that is finally dissolved in water of heat to synthesis carbon dots, mainly from the fluorescence intensity of the carbon dots solution to synthesis
Influence is investigated.
The concentration of phloroglucin solution has an impact the fluorescence intensity of carbon dots solution, the concentration difference of the phloroglucin of discussion
For 1.35 mmol/L, 1.95 mmol/L, 2.25 mmol/L, 2.85 mmol/L, 3.8 mmol/L, 4.75 mmol/L, 5.7
To the influence of the fluorescence intensity of the carbon dots solution of synthesis during mmol/L.As a concentration of 2.85 mmol/L of phloroglucin, carbon dots
The fluorescence of solution is most strong, and final preferred concentration is 2.85 mmol/L.
The concentration of dilute sulfuric acid has an impact the fluorescence intensity of carbon dots solution, and the concentration of the dilute sulfuric acid of discussion is respectively 0.0045
mol/L、0.0075 mol/L、0.01 mol/L、0.015 mol/L、0.02 mol/L、0.03 mol/L、0.035 mol/L、
To the influence of the fluorescence intensity of the carbon dots solution of synthesis during 0.04 mol/L.As a concentration of 0.015 mol/L of dilute sulfuric acid, carbon
The fluorescence of point solution is most strong, and final preferred concentration is 0.015 mol/L.
The total volume of phloroglucin and dilute sulfuric acid also has certain influence to the fluorescence intensity of carbon dots solution, has inquired into isophthalic three
The total volume of phenol and dilute sulfuric acid is respectively 10 mL, 20 mL, 30 mL, 40 mL to the shadow of the fluorescence intensity of the carbon dots solution of synthesis
It rings.The fluorescence of carbon dots solution is stronger when the total volume of phloroglucin and dilute sulfuric acid is 10 mL, 20 mL, and when phloroglucin and
When the total volume of dilute sulfuric acid is 20 mL, the fluorescence of carbon dots solution is most strong, and final preferred volume is 20 mL.
Microwave firepower has an impact the fluorescence intensity of carbon dots solution.Probed into microwave firepower be respectively it is low fire, in it is low fire, in
Influence when fiery, middle high fire, high fire to the fluorescence intensity for synthesizing carbon dots solution.When microwave firepower is high fiery, middle high fire, carbon dots
The fluorescence of solution is stronger, and when microwave firepower is middle high fire, the fluorescence of carbon dots solution is most strong, during final preferably microwave firepower is
Gao Huo.
After microwave synthesis carbon dots, the volume of the water added when being finally dissolved in water also has centainly the fluorescence intensity of carbon dots solution
It influences, to the shadow of the carbon dots fluorescence intensity of synthesis when the volume for having inquired into solvent is respectively 5 mL, 10 mL, 15 mL, 20 mL
It rings.When the volume of solvent is 15 mL, the fluorescence of carbon dots solution is most strong, and final preferred solvent volume is 15 mL.
（3）Carbon dots are to the detection parameters of pH value of solution
Take the centrifuge tube of 7 2.0 mL, put on respectively A, B, C, D, E, F, No. G, 1.8 mL are added in into A-G centrifuge tubes and are shifted to an earlier date
25 times of carbon dots solution was diluted, then the Britton-Robinson of 200 μ L difference pH value is sequentially added into A-G centrifuge tubes
Buffer solution, pH value are respectively 1.81,2.56,2.87,3.29,4.35,5.33,5.72.Under conditions of 4 DEG C, wait to react
After 70 min, the solution in each centrifuge tube is tested in sepectrophotofluorometer successively, record carbon dots are in different pH value
Fluorescence spectrum value in the presence of BR buffer solutions, is as a result shown in Fig. 4, fluorescence intensity correlation ratio to several ㏒ (I F /I F0 ) and solution
PH value between quantitative relationship be：㏒(I F /I F0 ) = -0.9283+0.3070pH (r=0.9933)。
It should also be noted that, specific embodiments of the present invention are used only to exemplary illustration, do not limit in any way
Determining protection scope of the present invention, the related technical personnel of this field can be improved or changed according to some above-mentioned explanations, but
All these improvements and changes should all belong to the protection domain of the claims in the present invention.
Claims (10)
- A kind of 1. method that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, it is characterised in that including step Suddenly：(1) using phloroglucin as carbon source, the thick solution of carbon dots is synthesized under microwave heating condition, is obtained most after the processing such as centrifuging, filtering Whole carbon dots solution；(2) carbon dots solution and its fluorescence intensity from system after the BR buffer solutions reaction of different pH value are detected；(3) According to the relationship between the pH value of system and the logarithm of the fluorescence correlation ratio of carbon dots solution, solution can be detected pH。
- 2. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：Step (1) is described using phloroglucin as carbon source, and the process of carbon dots solution is synthesized under microwave heating condition and is：It will match The phloroglucin solution put is mixed in a certain ratio, then mixed solution is heated with certain density dilute sulfuric acid, reaction It is afterwards the thick solution of carbon dots with water dissolution.
- 3. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The totality of a concentration of 3.0 mmol/L of phloroglucin, a concentration of 1mol/L of sulfuric acid, phloroglucin and dilute sulfuric acid Product is 20 mL.
- 4. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：Mixed solution is placed in microwave heating treatment in micro-wave oven in step (1), firepower is middle high fire.
- 5. the method according to claim 4 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The microwave heating treatment time is 10 min.
- 6. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The processing of step (1) carbon dots solution：First by the thick solution of obtained carbon dots be respectively placed in centrifuge tube carry out at a high speed from The heart detaches, then obtained supernatant carried out to be filtered under diminished pressure processing, finally just obtains the transparent carbon dots solution of brown color.
- 7. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The centrifugal speed of the operation of the centrifugal treating of the thick solution of carbon dots of step (1) described acquisition is 10000 revs/min Clock, centrifugation time are 10 minutes.
- 8. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The ranging from 1.81-5.72 of pH value of solution can be detected.
- 9. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The carbon dots average grain diameter of synthesis is：2.90 nm.
- 10. the method according to claim 1 that pH value of solution is detected using phloroglucin as carbon source microwave Fast back-projection algorithm carbon dots, It is characterized in that：The carbon dots of synthesis have fluorescent characteristic, and maximum excitation wavelength is 365 nm, and maximum emission wavelength is 465 nm.
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| CN109324028A (en) * | 2018-11-19 | 2019-02-12 | 湖南科技大学 | A method of Cr (VI) is detected using ethylenediamine and nitric acid as raw material microwave rapid synthesis carbon dots solution |
| CN110117492A (en) * | 2019-04-17 | 2019-08-13 | 长春工业大学 | A kind of fluorescent carbon point and the preparation method and application thereof |
| CN111349324A (en) * | 2020-04-17 | 2020-06-30 | 广安长明高端产业技术研究院 | Fluorescent polylactic acid composite material and preparation method thereof |
| CN112174111A (en) * | 2020-09-30 | 2021-01-05 | 湖南科技大学 | Preparation method and application of near-infrared light-emitting carbon dots with p-phenylenediamine as carbon source |
| CN112940720A (en) * | 2021-02-01 | 2021-06-11 | 郑州大学 | Nitrogen-doped carbon nanodot with high luminous efficiency and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109324028A (en) * | 2018-11-19 | 2019-02-12 | 湖南科技大学 | A method of Cr (VI) is detected using ethylenediamine and nitric acid as raw material microwave rapid synthesis carbon dots solution |
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| CN110117492B (en) * | 2019-04-17 | 2021-12-10 | 长春工业大学 | Fluorescent carbon dot and preparation method and application thereof |
| CN111349324A (en) * | 2020-04-17 | 2020-06-30 | 广安长明高端产业技术研究院 | Fluorescent polylactic acid composite material and preparation method thereof |
| CN112174111A (en) * | 2020-09-30 | 2021-01-05 | 湖南科技大学 | Preparation method and application of near-infrared light-emitting carbon dots with p-phenylenediamine as carbon source |
| CN112940720A (en) * | 2021-02-01 | 2021-06-11 | 郑州大学 | Nitrogen-doped carbon nanodot with high luminous efficiency and preparation method thereof |
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